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A kind of preparation method of perfluoroalkane

A technology for perfluoroalkane and octane is applied in the field of preparation of perfluoroalkane, which can solve the problems of difficulty in controlling the temperature of a reactor uniformly, being unsuitable for mass production, and not being able to be continuously carried out, and achieving easy control of reaction conditions and yield. High, productivity-enhancing effect

Active Publication Date: 2015-08-19
苏州工业园区捷仕通医疗设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cobalt trifluoride method needs to convert cobalt difluoride into cobalt trifluoride by fluorination first, and then cobalt trifluoride reacts with octane in the reactor to obtain a mixture containing perfluorooctane; cobalt trifluoride needs to be continuously regenerated , the reactor temperature is difficult to control uniformly, the scale-up is limited, the production cannot be carried out continuously, and it is not suitable for mass production
In addition, the electrolytic fluorination method to synthesize perfluorooctane has complex equipment, difficult condition control, many by-products, and low yield, which generally does not exceed 15%.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0031] A monel alloy reactor with an inner diameter of 80 mm and a length of 1000 mm is filled with spherical alumina with a diameter of Φ3 mm. The reactor is heated to 300°C, and a 50% fluorine-50% nitrogen mixture gas is introduced for fluorination, so that the alumina is completely converted into aluminum fluoride. Then keep the temperature of the reactor at 200°C, continuously feed 20% fluorine-nitrogen mixed gas and 10% octane-nitrogen mixed gas at the molar ratio of fluorine to octane 20:1 for reaction, and control the residence time for 5 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and dry it with anhydrous sodium sulfate After rectification and separation, the fraction with a boiling point of 100-105°C was taken to obtain 1000 grams of perfluorooc...

Embodiment 2

[0033] Use the same equipment as in Example 1. The temperature of the reactor is maintained at 260°C, and 20% fluorine-nitrogen mixed gas and 20% octane-nitrogen mixed gas are continuously fed into the reaction according to the ratio of fluorine gas to octane molar ratio of 20:1, and the residence time is controlled for 10 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and dry it with anhydrous sodium sulfate Afterwards, rectification and separation were carried out, and the fraction with a boiling point of 100-105°C was taken to obtain 1500 grams of perfluorooctane with a purity of 98.5% and a yield of about 75%.

Embodiment 3

[0035] Use the same equipment as in Example 1. The temperature of the reactor is maintained at 280°C, and 20% fluorine-nitrogen mixed gas and 15% octane-nitrogen mixed gas are continuously fed into the reaction according to the molar ratio of fluorine gas to octane of 25:1, and the residence time is controlled for 10 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and dry it with anhydrous sodium sulfate Afterwards, rectification and separation were carried out, and the fraction with a boiling point of 100-105°C was taken to obtain 1600 grams of perfluorooctane with a purity of 98% and a yield of about 65%.

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Abstract

The invention provides a method for preparing perfluoroalkane. The method comprises the following steps of: filling a filler in a reactor, fluorating by using a fluorating agent, keeping the temperature inside the reactor between 100 to 300 DEG C, adding reaction materials in a vaporizer to vaporize, controlling the temperature inside the vaporizer between 130 to 150 DEG C, wherein the reaction materials comprise C5-C16 alkanes and one or more of partial fluorides of the C5-C16 alkanes, continuously bringing reaction material vapor in the reactor by using an inert gas, continuously feeding the fluorating agent in the reactor to react with the reaction material vapor continuously fed in the reactor, and separating and purifying to obtain the perfluoroalkane. The method provided by the invention is suitable for large-scale continuous productions; the reaction conditions are easily controlled; the yield is high; the by-products are less; the reaction production is easily separated and purified; no three wastes are discharged during the production process. With the adoption of the method, perfluorooctane with the purity being greater than or equal to 98% can be prepared and can act as a production material of lung cavity ventilation aerating liquid and a preparation for ophthalmologic operations.

Description

technical field [0001] The invention relates to a preparation method of perfluoroalkane, in particular to a lung cavity ventilation liquid and a preparation method thereof. Background technique [0002] In the past, the preparation methods of perfluorooctane include cobalt trifluoride fluorination method and electrolytic fluorination method. The cobalt trifluoride method needs to convert cobalt difluoride into cobalt trifluoride by fluorination first, and then cobalt trifluoride reacts with octane in the reactor to obtain a mixture containing perfluorooctane; cobalt trifluoride needs to be continuously regenerated , the temperature of the reactor is difficult to control uniformly, the scale-up is limited, the production cannot be carried out continuously, and it is not suitable for mass production. In addition, the electrolytic fluorination method to synthesize perfluorooctane has complex equipment, difficult condition control, many by-products, and low yield, which general...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/08C07C17/10A61K31/02A61P11/00
Inventor 鲁俞方治文
Owner 苏州工业园区捷仕通医疗设备有限公司
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